CN101475557A - Preparation of high purity and high optical rotation mixing vitamin E - Google Patents
Preparation of high purity and high optical rotation mixing vitamin E Download PDFInfo
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- CN101475557A CN101475557A CNA2009100776384A CN200910077638A CN101475557A CN 101475557 A CN101475557 A CN 101475557A CN A2009100776384 A CNA2009100776384 A CN A2009100776384A CN 200910077638 A CN200910077638 A CN 200910077638A CN 101475557 A CN101475557 A CN 101475557A
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Abstract
The invention discloses a method for preparing a high-purity and high-optical rotation mixed vitamin E, which comprises the following steps: dissolving a low-content mixed vitamin E into ethanol water; carrying out absorptive separation of anion exchange resin; adding ethanol water into the mixed solution till an effluent is colorless; passing an acidic gas through the mixed solution for analysis; eluting with the ethanol water and concentrating an eluate; adding first-grade edible oil into a concentrate of the eluate with mixing; and subjecting the mixture to three-stage molecular distillation and obtaining the high-purity and high-optical rotation vitamin E. The method overcomes the separation difficulty caused by a plurality of solvents adopted, reduces production cost, simplifies operation, tremendously enhances the color and luster of products, greatly reduces the content of sterol in the raw material, and improves the product purity, optical rotation fluidity and transparency. The products have almost no residual solvent and can be used more safely in food industry and other industries.
Description
Technical field
The present invention relates to a kind of preparation method of vitamin-E, particularly relate to the preparation method of a kind of high purity, high optical rotation mixing vitamin E.
Background technology
Natural VE belongs to the ester soluble vitamin, mainly be that the deodorization distillate (being called for short DD oil) that obtains from the vegetable oil refining process is converted into fatty acid methyl ester by esterification and transesterify with free fatty acids and neutral oil, remove most of sterol by cold crystallization again, the process molecular distillation separates and obtains then, but purity is lower, generally at 30-50%.Natural VE is a kind of vitamin-E of mixed type, mainly is made up of α, β, four kinds of isomer of γ, δ.All about 50%, poor transparency and specific rotation are little for the natural VE purity of present domestic most of manufacturer production.Its major cause is that the existence by micromolecular neutral oil and sterol has influenced its purity, transparency and purity.The patent that relevant natural VE from low levels extracts high-load natural VE is a lot, and these methods cut both ways, and the quantity of solvent that has is big and the solvent kind is more, the product color that has is bad, and the yield that has is on the low side, is not suitable for suitability for industrialized production, the residual molten height of product, safety in utilization is low.
CN1401644A discloses a kind of method that obtains the high purity mixed tocopherol by steps such as fixed bed esterification, fractionation by adsorption, subzero fractionation and solvent extractions, this method uses the solvent kind more, causes the separated from solvent difficulty, and production cost is higher, product color is relatively poor, the residual molten height of product.
CN1440969A discloses raw material obtains the high purity mixed tocopherol by esterification, saponification, esterification, freezing, short-path distillation and fractionation by adsorption method, two kinds of solvents have been used during this method fractionation by adsorption, cause difficulty for the separation of solvent, the residual molten height of product is unfavorable for production control and poor stability.
CN101323607A discloses raw material and has separated the method that obtains the high purity mixed tocopherol with silica gel column chromatography by esterification alcoholysis, freezing, short-path distillation, this method has been used two kinds of solvents equally when silica gel column chromatography separates, cause difficulty for the separation of solvent, the residual molten height of product adopts multistage to separate and is unfavorable for production control and poor stability.
Summary of the invention
The objective of the invention is to overcome the deficiency that the multiple solvent of available technology adopting causes the separated from solvent difficulty, a kind of high purity of single solvent, preparation method of high optical rotation mixing vitamin E of adopting is provided.
Technical scheme of the present invention is summarized as follows:
The preparation method of a kind of high purity, high optical rotation mixing vitamin E comprises the steps:
(1) with the quality percentage composition of 1 parts by volume in the concentration expressed in percentage by volume that 10%～50% mixing vitamin E joins 0.5～4 parts by volume is 95%～100% aqueous ethanolic solution, 25～50 ℃ of fully dissolvings down;
(2) solution that the described step (1) of 0.5～3 times of anionite-exchange resin volume is obtained carries out fractionation by adsorption by anionite-exchange resin, and adsorption time was at 1～6 hour, and effluent liquid removes to reclaim ethanol;
(3) adding concentration expressed in percentage by volume in the anionite-exchange resin after absorption is 95%～100% aqueous ethanolic solution, treats that effluent liquid is till colourless;
(4) feed sour gas to resolving through the anionite-exchange resin of step (3), gaseous tension is controlled at 0.01～0.3MPa, and the time was at 10 minutes～2 hours;
(5) be that 95～100% aqueous ethanolic solution carries out wash-out with concentration expressed in percentage by volume again, collect elutriant, to elutriant be colourless till;
(6) under vacuum condition, 60～70 ℃ elutriant is concentrated into no ethanol till, the elutriant enriched material;
(7) add first-grade edible oil in the elutriant enriched material, mix, the interpolation quality of described first-grade edible oil is 2%～8% of a described elutriant enriched material quality;
(8) mixture that step (7) is obtained carries out three grades of molecule distillation processing, and first class pressure is 100～500Pa, and temperature is 100～120 ℃, sloughs the light constituent material; Secondary pressure is 1～5Pa, and temperature is 170～220 ℃, and three stage pressures are 1～5Pa, and temperature is 170～220 ℃, obtains a kind of high purity, high optical rotation mixing vitamin E.
The model of described anionite-exchange resin is preferred: 201*7, JK206, HZ202, HY-2002.
Described sour gas is carbonic acid gas or sulfurous gas.
Described first-grade edible oil is one-level soybean oil or one-level rapeseed oil.
Present method has overcome the separation difficulty that exists behind the multiple solvent of available technology adopting, reduced production cost, simplified operation, greatly the taken on a new look color and luster of product greatly reduces the content of sterol in the raw material, and product purity reaches more than 95%, improved the specific rotation (specific rotatory power reach+more than 24 °) of product, improved the flowability and the transparency of product, the residual quantity of solvent is almost nil in the product, uses safer in industries such as food.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
The preparation method of a kind of high purity, high optical rotation mixing vitamin E comprises the steps:
(1) with the 150 mixing vitamin E (VE:47.52% (w/w) that restrain, sterol: 9.15% (w/w), other: 43.65% (w/w), specific rotatory power is for+17 °) to join the 300ml concentration expressed in percentage by volume be in 95% the aqueous ethanolic solution, 35 ℃ of fully dissolvings down;
(2) (adsorption column: φ 20mm*800mm) carry out fractionation by adsorption, adsorption time was at 2 hours, and effluent liquid removes to reclaim ethanol by anionite-exchange resin JK206 for the solution that the described step (1) of 2 times of anionite-exchange resin volumes is obtained;
(3) adding concentration expressed in percentage by volume in the anionite-exchange resin after absorption is 95% aqueous ethanolic solution, treats that effluent liquid is till colourless; Collect effluent liquid and remove to concentrate recovery ethanol;
(4) feed carbon dioxide to resolving through the anionite-exchange resin of step (3), gaseous tension is controlled at 0.1MPa, and the time was at 10 minutes;
(5) be that 95% aqueous ethanolic solution carries out wash-out with concentration expressed in percentage by volume again, collect elutriant, to elutriant be colourless till;
(6) under vacuum condition, 60 ℃ elutriant is concentrated into no ethanol till, elutriant enriched material 74.52 grams (VE:88.05%, sterol: 1.12%, other: 10.83%), color is opaquer;
(7) add the one-level soybean oil in the elutriant enriched material, mix, the interpolation quality of described one-level soybean oil is 5% of a described elutriant enriched material quality;
(8) mixture that step (7) is obtained carries out three grades of molecule distillation processing, and first class pressure is 200Pa, and temperature is 100 ℃, sloughs the light constituent material; Secondary pressure is 1Pa, temperature is 180 ℃, three stage pressures are 1Pa, temperature is 180 ℃, obtains a kind of high purity, high optical rotation mixing vitamin E 65.46 gram (VE:98.23%, sterols: 1.05%, other: 0.72%, specific rotatory power is+28 °), product is red transparent, the thickness oily liquids of good fluidity.The molecular distillation yield is 98%.
Anionite-exchange resin after absorption used is regenerated: the ethanolic soln that adds mass percentage concentration and be the ethanolic soln of 5% sodium hydroxide or mass percentage concentration in anionite-exchange resin and be 5% potassium hydroxide, the volume that adds is 2～4 times of anionite-exchange resin volume, the concentration expressed in percentage by volume that adds 2～4 times of anionite-exchange resin volumes again is 95% aqueous ethanolic solution, eject sodium hydroxide solution or potassium hydroxide solution in the anionite-exchange resin, to the pH value of effluent liquid be till 7, anionite-exchange resin can reuse.
The effluent liquid that step (2) and step (3) obtain collects, and can reclaim ethanol, recycles.
Embodiment 2
The preparation method of a kind of high purity, high optical rotation mixing vitamin E comprises the steps:
(1) with the quality percentage composition of 1 parts by volume in the concentration expressed in percentage by volume that 10% mixing vitamin E joins 0.5 parts by volume is 100% ethanol, 25 ℃ of fully dissolvings down;
(2) solution that the described step (1) of 0.5 times of anionite-exchange resin volume is obtained carries out fractionation by adsorption by anionite-exchange resin (model HZ202), and adsorption time was at 1 hour, and effluent liquid removes to reclaim ethanol;
(3) adding concentration expressed in percentage by volume in the anionite-exchange resin after absorption is 100% ethanol, treats that effluent liquid is till colourless;
(4) feed carbon dioxide to resolving through the anionite-exchange resin of step (3), gaseous tension is controlled at 0.01MPa, and the time was at 2 hours;
(5) be that 100% aqueous ethanolic solution carries out wash-out with concentration expressed in percentage by volume again, collect elutriant, to elutriant be colourless till;
(6) under vacuum condition, 70 ℃ elutriant is concentrated into no ethanol till, the elutriant enriched material;
(7) add the one-level soybean oil in the elutriant enriched material, mix, the interpolation quality of described one-level soybean oil is 2% of a described elutriant enriched material quality;
(8) mixture that step (7) is obtained carries out three grades of molecule distillation processing, and first class pressure is 500Pa, and temperature is 120 ℃, sloughs the light constituent material; Secondary pressure is 5Pa, and temperature is 220 ℃, and three stage pressures are 5Pa, and temperature is 220 ℃, obtains a kind of high purity, high optical rotation mixing vitamin E.
Embodiment 3
The preparation method of a kind of high purity, high optical rotation mixing vitamin E comprises the steps:
(1) with the quality percentage composition of 1 parts by volume in the concentration expressed in percentage by volume that 50% mixing vitamin E joins 4 parts by volume is 95% aqueous ethanolic solution, 50 ℃ of fully dissolvings down;
(2) solution that the described step (1) of 3 times of anionite-exchange resin volumes is obtained carries out fractionation by adsorption by anionite-exchange resin (model 201*7), and adsorption time was at 6 hours, and effluent liquid removes to reclaim ethanol;
(3) adding concentration expressed in percentage by volume in the anionite-exchange resin after absorption is 95% aqueous ethanolic solution, treats that effluent liquid is till colourless;
(4) feed sulfur dioxide gas to resolving through the anionite-exchange resin of step (3), gaseous tension is controlled at 0.3MPa, and the time was at 10 minutes;
(5) be that 95% aqueous ethanolic solution carries out wash-out with concentration expressed in percentage by volume again, collect elutriant, to elutriant be colourless till;
(6) under vacuum condition, 60 ℃ elutriant is concentrated into no ethanol till, the elutriant enriched material;
(7) add the one-level rapeseed oil in the elutriant enriched material, mix, the interpolation quality of described one-level rapeseed oil is 8% of a described elutriant enriched material quality;
(8) mixture that step (7) is obtained carries out three grades of molecule distillation processing, and first class pressure is 100Pa, and temperature is 100 ℃, sloughs the light constituent material; Secondary pressure is 1Pa, and temperature is 170 ℃, and three stage pressures are 1Pa, and temperature is 170 ℃, obtains a kind of high purity, high optical rotation mixing vitamin E.
Embodiment 4
The preparation method of a kind of high purity, high optical rotation mixing vitamin E comprises the steps:
(1) with the quality percentage composition of 1 parts by volume in the concentration expressed in percentage by volume that 30% mixing vitamin E joins 3 parts by volume is 98% aqueous ethanolic solution, 35 ℃ of fully dissolvings down;
(2) solution that the described step (1) of 2 times of anionite-exchange resin volumes is obtained carries out fractionation by adsorption by anionite-exchange resin (model HY-2002), and adsorption time was at 4 hours, and effluent liquid removes to reclaim ethanol;
(3) adding concentration expressed in percentage by volume in the anionite-exchange resin after absorption is 98% aqueous ethanolic solution, treats that effluent liquid is till colourless;
(4) feed sulfur dioxide gas to resolving through the anionite-exchange resin of step (3), gaseous tension is controlled at 0.05MPa, and the time was at 1 hour;
(5) be that 98% aqueous ethanolic solution carries out wash-out with concentration expressed in percentage by volume again, collect elutriant, to elutriant be colourless till;
(6) under vacuum condition, 65 ℃ elutriant is concentrated into no ethanol till, the elutriant enriched material;
(7) add the one-level rapeseed oil in the elutriant enriched material, mix, the interpolation quality of described one-level rapeseed oil is 6% of a described elutriant enriched material quality;
(8) mixture that step (7) is obtained carries out three grades of molecule distillation processing, and first class pressure is 300Pa, and temperature is 110 ℃, sloughs the light constituent material; Secondary pressure is 3Pa, and temperature is 180 ℃, and three stage pressures are 3Pa, and temperature is 180 ℃, obtains a kind of high purity, high optical rotation mixing vitamin E.
Claims (4)
1. the preparation method of a high purity, high optical rotation mixing vitamin E is characterized in that comprising the steps:
(1) with the quality percentage composition of 1 parts by volume in the concentration expressed in percentage by volume that 10%～50% mixing vitamin E joins 0.5～4 parts by volume is 95%～100% aqueous ethanolic solution, 25～50 ℃ of fully dissolvings down;
(2) solution that the described step (1) of 0.5～3 times of anionite-exchange resin volume is obtained carries out fractionation by adsorption by anionite-exchange resin, and adsorption time was at 1～6 hour, and effluent liquid removes to reclaim ethanol;
(3) adding concentration expressed in percentage by volume in the anionite-exchange resin after absorption is 95%～100% aqueous ethanolic solution, treats that effluent liquid is till colourless;
(4) feed sour gas to resolving through the anionite-exchange resin of step (3), gaseous tension is controlled at 0.01～0.3MPa, and the time was at 10 minutes～2 hours;
(5) be that 95～100% aqueous ethanolic solution carries out wash-out with concentration expressed in percentage by volume again, collect elutriant, to elutriant be colourless till;
(6) under vacuum condition, 60～70 ℃ elutriant is concentrated into no ethanol till, the elutriant enriched material;
(7) add first-grade edible oil in the elutriant enriched material, mix, the interpolation quality of described first-grade edible oil is 2%～8% of a described elutriant enriched material quality;
(8) mixture that step (7) is obtained carries out three grades of molecule distillation processing, and first class pressure is 100～500Pa, and temperature is 100～120 ℃, sloughs the light constituent material; Secondary pressure is 1～5Pa, and temperature is 170～220 ℃, and three stage pressures are 1～5Pa, and temperature is 170～220 ℃, obtains a kind of high purity, high optical rotation mixing vitamin E.
2. the preparation method of a kind of high purity according to claim 1, high optical rotation mixing vitamin E is characterized in that the model of described anionite-exchange resin is: 201*7, JK206, HZ202, HY-2002.
3. the preparation method of a kind of high purity according to claim 1, high optical rotation mixing vitamin E is characterized in that described sour gas is carbonic acid gas or sulfurous gas.
4. the preparation method of a kind of high purity according to claim 1, high optical rotation mixing vitamin E is characterized in that described first-grade edible oil is one-level soybean oil or one-level rapeseed oil.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104130233A (en) * | 2014-07-03 | 2014-11-05 | 山东圣地嘉禾生物工程有限公司 | Method for preparing natural alpha tocopherol and mixing tocopherol by one-step method |
| CN105985308A (en) * | 2015-02-15 | 2016-10-05 | 浙江医药股份有限公司新昌制药厂 | Method for simultaneously preparing high-content mixed tocopherols and d-delta-tocopherol monomer |
| CN104130233B (en) * | 2014-07-03 | 2016-11-30 | 山东圣地嘉禾生物工程有限公司 | One-step method prepares the method for natural alpha tocopherol and mixed tocopherol |
| CN110283034A (en) * | 2019-07-12 | 2019-09-27 | 陕西海斯夫生物工程有限公司 | A method of obtaining high-purity squalene from plant oil deodorizing distillate |
| CN114644609A (en) * | 2020-12-18 | 2022-06-21 | 丰益生物科技(江苏)有限公司 | Method for extracting natural vitamin E from byproduct residual oil |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1092703A (en) * | 1966-04-05 | 1967-11-29 | Eisai Co Ltd | Process of isolating and refining tocopherol homologues |
| CN101074258B (en) * | 2007-06-14 | 2010-04-21 | 河北科技大学 | Method for separating and extracting phytosterin and Vitamin E from soyabean deodorization distillate |
-
2009
- 2009-02-10 CN CN2009100776384A patent/CN101475557B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104130233A (en) * | 2014-07-03 | 2014-11-05 | 山东圣地嘉禾生物工程有限公司 | Method for preparing natural alpha tocopherol and mixing tocopherol by one-step method |
| CN104130233B (en) * | 2014-07-03 | 2016-11-30 | 山东圣地嘉禾生物工程有限公司 | One-step method prepares the method for natural alpha tocopherol and mixed tocopherol |
| CN105985308A (en) * | 2015-02-15 | 2016-10-05 | 浙江医药股份有限公司新昌制药厂 | Method for simultaneously preparing high-content mixed tocopherols and d-delta-tocopherol monomer |
| CN110283034A (en) * | 2019-07-12 | 2019-09-27 | 陕西海斯夫生物工程有限公司 | A method of obtaining high-purity squalene from plant oil deodorizing distillate |
| CN110283034B (en) * | 2019-07-12 | 2022-04-12 | 陕西海斯夫生物工程有限公司 | Method for obtaining high-purity squalene from vegetable oil deodorized distillate |
| CN114644609A (en) * | 2020-12-18 | 2022-06-21 | 丰益生物科技(江苏)有限公司 | Method for extracting natural vitamin E from byproduct residual oil |
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